CN101810262A - Xylitol mother liquor crystallization method - Google Patents
Xylitol mother liquor crystallization method Download PDFInfo
- Publication number
- CN101810262A CN101810262A CN200910014321A CN200910014321A CN101810262A CN 101810262 A CN101810262 A CN 101810262A CN 200910014321 A CN200910014321 A CN 200910014321A CN 200910014321 A CN200910014321 A CN 200910014321A CN 101810262 A CN101810262 A CN 101810262A
- Authority
- CN
- China
- Prior art keywords
- massecuite
- xylitol
- mother liquor
- freezing
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 39
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 title claims abstract description 39
- 229960002675 xylitol Drugs 0.000 title claims abstract description 39
- 239000000811 xylitol Substances 0.000 title claims abstract description 39
- 239000012452 mother liquor Substances 0.000 title claims abstract description 26
- 238000002425 crystallisation Methods 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 22
- 230000008014 freezing Effects 0.000 claims abstract description 22
- 238000007710 freezing Methods 0.000 claims abstract description 22
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 4
- 238000004094 preconcentration Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- MSXHSNHNTORCAW-GGLLEASOSA-M sodium;(2s,3s,4s,5r,6s)-3,4,5,6-tetrahydroxyoxane-2-carboxylate Chemical compound [Na+].O[C@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O MSXHSNHNTORCAW-GGLLEASOSA-M 0.000 claims description 6
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 229940069338 potassium sorbate Drugs 0.000 claims description 3
- 235000010241 potassium sorbate Nutrition 0.000 claims description 3
- 239000004302 potassium sorbate Substances 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 3
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229960003487 xylose Drugs 0.000 description 1
Abstract
The invention discloses a xylitol mother liquor crystallization method, belonging to the technical field of functional sugar production. The crystallization method adds three steps of dehydration promotion, room-temperature placement and freezing crystallization on the basis of the traditional crystallization method, adopts a dehydrating agent and a accelerator, and comprises the following specific technical steps: (1) prethickening; (2) dehydration promotion; (3) cooling crystallization; (4) displacing at room temperature; (5) freezing crystallization; (6) decentralizing; and (7) drying, packaging and the like. The crystallization method of the invention solves the problem of difficult crystallization of xylitol mother liquor, improves yield, fully utilizes raw materials, improves purity and quality of xylitol crystals, and improves the additional value of the xylitol mother liquor. The invention is also suitable for xylitol crystallization.
Description
Technical field
The invention belongs to technical field of functional sugar production, relate to a kind of method for crystallising of Xylitol mother liquor.
Background technology
Xylitol is to be obtained by the wood sugar hydrogenation, and xylitol solution is through purification, evaporation, vacuum crystallization, the centrifugal xylitol crystal that obtains.In the xylitol production traditional vacuum method for crystallising be with the massecuite pre-concentration to hypersaturated state, add crystal seed, vacuum cool-down crystallization, the centrifugal crystal that obtains.Can produce a large amount of Xylitol mother liquors in the crystal xylitol is produced, Xylitol mother liquor is because impurity is many, purity is low, adopts the method for traditional vacuum crystallization can not obtain crystal, and Xylitol mother liquor can only use as liquid xylitol.Liquid xylitol brings very big inconvenience for storage and transportation, because purity is low, range of application also is restricted, and added value is lower.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of Xylitol mother liquor crystallization method, can not obtain crystal to solve prior art, can only use as liquid xylitol, because problem such as purity is low, and range of application also is restricted, and added value is lower.
The technical scheme that the present invention is adopted for its technical problem of solution provides a kind of method for crystallising of new Xylitol mother liquor, dehydration promotion, room temperature placement, three steps of freezing and crystallizing on the basis of conventional junction crystal method, have been increased, and added dehydrating agent and promoter, this method for crystallising is made up of following processing step:
1, pre-concentration: it is 75-95% that the Xylitol mother liquor vacuum is concentrated into concentration.
2, dehydration promotes: the cooling of the massecuite after step 1 pre-concentration is cooled to temperature when being 44-52 ℃, the 0.1-5% that presses massecuite unit weight adds one or both in glycerine, the absolute ethyl alcohol, press the 0.01-0.10% adding gluconic acid sodium salt of massecuite dry weight, in the potassium sorbate one or both.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, about 45 ℃ of temperature, the 0.2-0.8% that presses the massecuite dry weight adds xylitol micro powders, decrease temperature crystalline 10-36 hour, proper extension temperature fall time.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 16-32 hour, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 8-72 hour.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Adopt this method, solved the problem of Xylitol mother liquor crystallization difficulty, improved yield, raw material is fully used, improved the purity and the quality of xylitol crystal, improved the added value of Xylitol mother liquor.The present invention is equally applicable to the xylitol crystallization.
Specific embodiment
Get Xylitol mother liquor 1000g, several different modes with reference to adding dehydrating agent and promoter provide following concrete embodiment.
Embodiment 1
1, pre-concentration: get Xylitol mother liquor 1000g, it is 75% that vacuum is concentrated into concentration.
2, dehydration promotes: the cooling of the massecuite after step 1 pre-concentration is cooled to temperature when being 50 ℃, adds absolute ethyl alcohol 0.58ml, add gluconic acid sodium salt 0.14g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, when 44 ℃ of temperature, add xylitol micro powders 3.9g, decrease temperature crystalline 10 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 24 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed the later massecuite of crystallization, be put in 4 ℃ of refrigerators freezing and crystallizing 39 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Embodiment 2
1, pre-concentration: get Xylitol mother liquor 1000g, it is 78% that vacuum is concentrated into concentration.
2, dehydration promotes: the cooling of the massecuite after step 1 pre-concentration is cooled to temperature when being 50 ℃, adds absolute ethyl alcohol 0.4ml, add glycerine 0.2ml, add gluconic acid sodium salt 0.24g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, about 45 ℃ of temperature, add xylitol micro powders 3g, decrease temperature crystalline 11 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 15.5 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 16 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Embodiment 3
1, pre-concentration: get Xylitol mother liquor 1000g, it is 78% that vacuum is concentrated into concentration.
2, dehydration promotes: the cooling of the massecuite after step 1 pre-concentration is cooled to temperature when being 45 ℃, adds absolute ethyl alcohol 44ml, add gluconic acid sodium salt 0.1g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, when 44 ℃ of temperature, add xylitol micro powders 2.34g, decrease temperature crystalline 10 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 16 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 56 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Embodiment 4
1, pre-concentration: get Xylitol mother liquor 1000g, it is 80% that vacuum is concentrated into concentration.
2, dehydration promotes: the cooling of the massecuite after step 1 pre-concentration is cooled to temperature when being 46 ℃, adds absolute ethyl alcohol 4ml, add gluconic acid sodium salt 0.2g, add potassium sorbate 0.07g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, when 46 ℃ of temperature, add xylitol micro powders 4.44g, decrease temperature crystalline 26 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 32 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 38 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Claims (1)
1. an Xylitol mother liquor crystallization method is characterized in that having increased dehydration promotion, room temperature placement, three steps of freezing and crystallizing, and has added dehydrating agent and promoter on the basis of conventional junction crystal method, and this method for crystallising is made up of following processing step:
(1) pre-concentration: it is 75-95% that the Xylitol mother liquor vacuum is concentrated into concentration;
(2) dehydration promotes: the cooling of the massecuite after step 1 pre-concentration is cooled to temperature when being 44-52 ℃, the 0.1-5% that presses massecuite unit weight adds one or both in glycerine, the absolute ethyl alcohol, press the 0.01-0.10% adding gluconic acid sodium salt of massecuite dry weight, in the potassium sorbate one or both;
(3) decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, about 45 ℃ of temperature, the 0.2-0.8% that presses the massecuite dry weight adds xylitol micro powders, decrease temperature crystalline 10-36 hour, proper extension temperature fall time;
(4) room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 16-32 hour, and massecuite bleaches, and crystal grain increases;
(5) freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 8-72 hour;
(6) centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal;
(7) drying and packaging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910014321A CN101810262B (en) | 2009-02-20 | 2009-02-20 | Xylitol mother liquor crystallization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910014321A CN101810262B (en) | 2009-02-20 | 2009-02-20 | Xylitol mother liquor crystallization method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101810262A true CN101810262A (en) | 2010-08-25 |
| CN101810262B CN101810262B (en) | 2012-09-19 |
Family
ID=42617752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910014321A Active CN101810262B (en) | 2009-02-20 | 2009-02-20 | Xylitol mother liquor crystallization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101810262B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103442583A (en) * | 2011-03-31 | 2013-12-11 | 日本卡夫食品株式会社 | Flowable food composition and confection |
| US10759727B2 (en) | 2016-02-19 | 2020-09-01 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
| CN111777493A (en) * | 2020-08-29 | 2020-10-16 | 浙江华康药业股份有限公司 | Xylitol mother liquor utilization system and method |
| CN116063158A (en) * | 2022-12-17 | 2023-05-05 | 浙江华康药业股份有限公司 | Induction nucleation crystallization method for improving anti-caking performance of xylitol |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1290812C (en) * | 2005-07-20 | 2006-12-20 | 天津市圭谷科技发展有限公司 | Method for extracting xylitol from xylitol mother liquor |
| CN1284755C (en) * | 2005-07-25 | 2006-11-15 | 天津大学 | Xylitol refining crystallization process |
| CN101200407B (en) * | 2007-12-07 | 2010-10-20 | 胡学仁 | Method for abstracting xylitol from by-product liquid of xylitol production |
-
2009
- 2009-02-20 CN CN200910014321A patent/CN101810262B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103442583A (en) * | 2011-03-31 | 2013-12-11 | 日本卡夫食品株式会社 | Flowable food composition and confection |
| CN103442583B (en) * | 2011-03-31 | 2015-09-09 | 亿滋日本株式会社 | Fluidity food compositions and confectionery |
| US10759727B2 (en) | 2016-02-19 | 2020-09-01 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
| US11840500B2 (en) | 2016-02-19 | 2023-12-12 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
| CN111777493A (en) * | 2020-08-29 | 2020-10-16 | 浙江华康药业股份有限公司 | Xylitol mother liquor utilization system and method |
| CN116063158A (en) * | 2022-12-17 | 2023-05-05 | 浙江华康药业股份有限公司 | Induction nucleation crystallization method for improving anti-caking performance of xylitol |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101810262B (en) | 2012-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106496159B (en) | A kind of production technology of the big granularity crystal of acesulfame potassium | |
| CN100357307C (en) | Crystallization method of abamectin Bla | |
| CN104072549B (en) | The production technique of Gastrodine | |
| CN101810262B (en) | Xylitol mother liquor crystallization method | |
| CN106045879B (en) | Method for preparing cyanoacetic acid | |
| WO2017080520A1 (en) | Method for extracting avermectin b2 from avermectin ointment | |
| CN104327100A (en) | Preparation technology of high-purity flomoxef sodium | |
| CN102476997B (en) | Method for preparing chlorogenic acid by freezing, concentrating and crystallizing | |
| CN104926709B (en) | A kind of process for purification of L tryptophans | |
| CN104513256A (en) | Preparation method of cefditoren pivoxil | |
| CN101156675A (en) | Glutamic acid abstraction technics combining rotation crystal | |
| CN103275047B (en) | Preparation method of griseofulvin | |
| CN101671283A (en) | Preparation method of columnar crystal taurine | |
| CN107652346B (en) | Method for treating cyproterone acetate ketal mother liquor | |
| CN112047999B (en) | Preparation method of gamma-crystal form arginine perindopril salt | |
| CN109400662B (en) | Crystallization method of abamectin | |
| CN101870704A (en) | Method for purifying cefotetan acid crude products | |
| CN101928220B (en) | Preparation method of 1-hydroxyl-2-naphthoate | |
| US10414776B2 (en) | Efficient method for producing and purifying anhydrous sugar alcohol | |
| CN100577675C (en) | Process for producing crystallized xylose by hydrolyzing corn skin | |
| CN110128487B (en) | Abamectin refining method | |
| CN115010599B (en) | Method for separating and refining salicylic acid from sodium salicylate acidified material | |
| CN102234225B (en) | Production method for citric acid monohydrate crystal | |
| CN101712615A (en) | Method for preparing crystal glyoxylic acid | |
| US20240101504A1 (en) | Hydroxyalkanoic acid crystal production method and hydroxyalkanoic acid crystal polymorph |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PP01 | Preservation of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20231114 Granted publication date: 20120919 |